Lab 1

Precipitation and Isolation of an Insoluble Lead Salt

1. Weigh the Sample

Top-loading balance

- Place weigh boat on balance and tare.

- Weigh out about 0.8g (0.7g to 0.9g) of the sample into the weigh boat.

Sample colour?

Analytical balance (Note the number or position of this balance for later)

- Weigh the boat + the sample again. (Handle weigh boat with paper to avoid oil staining)

Measurement 1 - (4 d.p.)

- Transfer sample to 250ml beaker.

- Weigh emptied weigh boat.

Measurement 2 - (4 d.p.)

Measurement 3 = Measurement 1 - Measurement 2 (4 d.p.)

2. Dissolve the Sample

- Boil 150ml deionised water at setting 3 on hot plate.

- Add 5ml of ethanoic (acetic) acid to the beaker.
- Add 50ml of the boiled deionized water to the beaker.
- Stir until sample is fully dissolved.
- Reheat to gentle boil.

Colour of solution of dissolved sample?

3. Precipitating the Lead Salt

- Remove beaker from hot plate using oven mitts.

- Add 2ml sodium sulfate, stirring continuously.
- Allow precipitate to settle for a few minutes.
- Cover beaker with watch glass and boil for 10 minutes.
- Cool beaker until cold enough to handle.

Colour of precipitate?
4. Isolating the Lead Salt

- Collect glass crucible from oven (using oven mitts) and place on tile.
- Cover with aluminium foil and mark your name.
- Let it cool to room temperature (don’t touch with bare hands).
- Remove crucible with paper and weigh using analytical balance.

Measurement 5 (not 4) - (4 d.p.)

- Remove crucible with paper from balance and screw it into vacuum adapter.
- Pour solution through crucible.
- Use wash bottle to transfer washings (repeat several times).
- Use rubber police man to transfer any precipitate on walls of container.
- Rinse precipitate with cold deionized water.
- Add anhydrous ethanol.
- Dry by suction for 2-3 minutes.
- After completion, break vacuum from plastic joint AND THEN close tap.
- Transfer crucible back to beaker with paper, cover with foil and poke a hole in the top.
- Place beaker with crucible into hot oven for about 30 minutes.

4. Weighing the Lead Salt

- Remove crucible with oven mitts and cool it by placing it into an ice bath.
- Weigh using the same analytical balance you used the first time.

Measurement 4 - (4 d.p.)

Measurement 6 = Measurement 4 - Measurement 5 (4 d.p.)

Colour of lead salt?

5. Clean - Up

- Scrape lead sulfate from filter crucible into marked waste bottle.
- Wash crucible using wire brush.
- Return crucible and accompanying beaker to Chemistry Stores counter.
  

Gravimetric Experiment 1 Online Tutorial >> Gravimetric Analysis >> Evaluation
Analysis Questions
­Introduction
­Precipitating the Pb2+   < Previous | Next >
ion
­How much Na2SO4 to
Name: Sahil Kanani     Student Number: A3101
add
­Amount of Pb2+ in the
sample Experiment 1 ­ Gravimetric Analysis
­Application Question
Evaluation Question 1
­Evaluation Questions
Part (a)

An impure potassium chloride sample weighing about 0.63 g
was dissolved in water. Calculate the volume of 1.5 M AgNO3
needed to completely precipitate the chloride ions. (Give your
answer to 2 significant figures.)

          5.63  mL AgNO3  Check Answer

Your answer is correct!

Please print this page and continue to the next problem.

Name: Sahil Kanani     Student Number: A3101

Part (b)

The unknown sample from Part (a) was found to have a mass
of 0.6333 g. The mass of silver chloride that precipitated was
0.8170 g. What is the percentage chloride in the unknown?
(Please give your answer to 4 significant figures)

          31.91  %  Check Answer

Your answer is correct!

Please print this page and continue to the next problem.

If you are unable to print, you can take a screen capture of
this page by following the instructions below: 
   1. Click the ’PrntScrn’ button on your keyboard. (The image
of the screen will be copied to the clipboard.)
   2. Open a new document in MS Word and press CTRL + V
to paste the image into your document. 
   3. You may then save the document to print when you
come to lab.

Contact Us Last Updated: Wednesday, August 17th, 2016 @ 11:17:37 am
  

Gravimetric Experiment 1 Online Tutorial >> Gravimetric Analysis >> Evaluation
Analysis Questions
­Introduction
­Precipitating the Pb2+   < Previous | Next >
ion
­How much Na2SO4 to
Name: Sahil Kanani     Student Number: A3101
add
­Amount of Pb2+ in the
sample Experiment 1 ­ Gravimetric Analysis
­Application Question
Evaluation Question 2
­Evaluation Questions
A 2.267 g sample of limestone was dissolved in HCl and all
the calcium in the limestone was converted to Ca2+(aq). The
solution was treated with excess ammonium oxalate,
(NH4)2C2O4(aq), and it was found that 2.300 g of calcium
oxalate, CaC2O4(s) was precipitated. Calculate the percentage
of calcium in the limestone. (Please give your answer to 4
significant figures)

          31.74  %  Check Answer

Your answer is correct!

Please print this page and continue to the next problem.

If you are unable to print, you can take a screen capture of
this page by following the instructions below: 
   1. Click the ’PrntScrn’ button on your keyboard. (The image
of the screen will be copied to the clipboard.)
   2. Open a new document in MS Word and press CTRL + V
to paste the image into your document. 
   3. You may then save the document to print when you
come to lab.

Contact Us Last Updated: Wednesday, August 17th, 2016 @ 11:17:37 am
  

Gravimetric Experiment 1 Online Tutorial >> Gravimetric Analysis >> Evaluation
Analysis Questions
­Introduction
­Precipitating the Pb2+   < Previous | Next >
ion
­How much Na2SO4 to
Name: Sahil Kanani     Student Number: A3101
add
­Amount of Pb2+ in the
sample Experiment 1 ­ Gravimetric Analysis
­Application Question
Evaluation Question 3
­Evaluation Questions
Part (a)

An impure barium chloride sample weighing about 0.39 g was
dissolved in water and then treated with excess sulfuric acid.
Calculate the volume of 4.0 M H2SO4 needed to completely
precipitate the barium ions as barium sulfate, BaSO4. (Give
your answer to 2 significant figures.)

          0.47  mL H2SO4  Check Answer

Your answer is correct!

Name: Sahil Kanani     Student Number: A3101

Part (b)

The impure barium chloride sample from Part (a) was found
to have a mass of 0.3869 g. The mass of barium sulfate,
BaSO4, that precipitated from the addition of sulfuric acid was
0.1593 g. What is the percentage barium in the unknown
sample? (Please give your answer to 4 significant figures)

          24.23  %  Check Answer

Your answer is correct!

Please print this page.

If you are unable to print, you can take a screen capture of
this page by following the instructions below: 
   1. Click the ’PrntScrn’ button on your keyboard. (The image
of the screen will be copied to the clipboard.)
   2. Open a new document in MS Word and press CTRL + V
to paste the image into your document. 
   3. You may then save the document to print when you
come to lab.

Contact Us Last Updated: Wednesday, August 17th, 2016 @ 11:17:38 am